CN103214237B - Preparation method of giant-dielectric-constant barium titanate ceramic - Google Patents
Preparation method of giant-dielectric-constant barium titanate ceramic Download PDFInfo
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Abstract
The invention relates to a preparation method of giant-dielectric-constant barium titanate ceramic, belonging to the technical field of ceramic materials. The giant-dielectric-constant barium titanate ceramic is sintered by using a self-propagating high-temperature quick pressurizing technology, wherein a self-propagating high-temperature system adopts a thermit system. The method comprises the following steps of: performing compression molding on barium titanate powder under the pressure of 200 MPa; placing into a self-propagating system; and after a self-propagating reaction is finished, applying axial pressure of 100 to 200 MPa, so that the barium titanate ceramic is compact. The barium titanate ceramic prepared by the method has the advantages of high dielectric constant, low dielectric loss and high heat stability. The self-propagating high-temperature quick pressurizing technology is low in energy consumption; the process is simple; the required materials are low in price; the sintering time is extremely short; and great value is achieved on industrial application.
Description
Technical field
The present invention relates to dielectric ceramic material and preparation method thereof, relate in particular to a kind of preparation method of huge dielectric constant barium titanate ceramics, belong to technical field of ceramic material.
Background technology
The molecular formula of barium titanate is BaTiO
3, be at room temperature Tetragonal, be a kind conventional ferroelectric material, there are good dielectric, piezoelectricity, ferroelectric properties, be widely used among electron device, as for the preparation of multiple electrical condenser, PTC thermistor, piezoelectric transducer, pyroelectric detector etc.Along with scientific-technical progress, the miniaturization of various device and microminiaturization have proposed requirements at the higher level to material property, various high dielectrics, and huge dielectric constant material is developed in succession.The specific inductivity of barium titanate ceramics is difficult to obtain higher lifting by general technology means, has therefore limited further developing of barium-titanate material.
As Chinese invention patent application (application number: 201110000663.X, the applying date: the sintering method that 2011-01-04) discloses a kind of increasing dielectric constant of barium titanate.The method with sol-gel method, prepare barium carbonate powder and in retort furnace sintering twice, prepared high-dielectric-constant ceramics, under the test condition that room temperature lower frequency is 100Hz, specific inductivity reaches 66724.The method thinks that the specific inductivity of barium titanate and inner domain structure have relation, can obtain maximum dielectric constant under optimum structure.Technique prepared by the method is comparatively complicated, prepare barium carbonate powder with sol-gel method, then with retort furnace, carry out sintering twice, and the cycle is longer, consumes energy larger, is not suitable for being applied to producing in enormous quantities.This pottery of what is more important can show high dielectric property under low frequency, but is that performance and applicability thereof under 1KHz is still unknowable in frequency.
As Chinese invention patent application (application number: 200510061081.7 applyings date: 2005-10-13) disclose a kind of temperature stability electronic ceramic material with ultra-high dielectric constant and preparation method thereof.Barium titanate by 80%～99%, 1%～5% acetylene black and 0%～15% PbO-B
2o
3after the ratio of glass powder is mixed; in agate mortar, grind or in grinding in ball grinder; take pressure as 2～10MPa compression moulding; the preparation of this stupalith need to be carried out under the protection of vacuum or shielding gas; prepared pottery has high-k; room temperature lower frequency is that under the test condition of 1KHz, specific inductivity reaches 45000, and dielectric loss is 69.5%.The method improves the dielectric properties of barium titanate ceramics with seepage theory, by add conductor in dielectric, when the volume content of conductor is near percolation threshold, non-linear enhancing can occur the specific inductivity of material.The goods specific inductivity of the method gained is not high, and dielectric loss is very large, and preparation technology is comparatively complicated, and power consumption is large.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of huge dielectric constant barium titanate ceramics.The method desired raw material kind is few, with low cost, and simple and low, the prepared barium titanate ceramics that consume energy of preparation technology have the advantage that specific inductivity is high, dielectric loss is low and thermostability is high.
To achieve these goals, the technical solution adopted in the present invention is:
A preparation method for huge dielectric constant barium titanate ceramics, is characterized in that, it comprises the following steps:
1) preparation is from spreading system powder
By weight percentage, take chromium sesquioxide powder 54%-62%, aluminium powder 19%-22%, carbon dust 5%-7%, aluminum oxide powder 10%-20%, carries out ball milling by load weighted chromium sesquioxide powder, aluminium powder, carbon dust, aluminum oxide powder after mixing, and obtains composite granule;
Composite granule is dried, and granulation, obtains granular composite granule;
2) prepare just base of barium titanate
Barium titanate powder is pressed into disk, then barium titanate disk is superscribed to graphite paper and boron nitride powder successively, be then pressed into just base of barium titanate;
3) self propagating high temperature Quick-pressing sintering:
The first base of barium titanate is positioned in the granular composite granule making through step 1), be pressed into column, described column is positioned in self propagating high temperature Quick-pressing equipment, self-propagating reaction ignites, and in the time of 40 seconds-70 seconds, apply the axle pressure of 100MPa-200MPa, pressurize 60 seconds, naturally cooling, obtains huge dielectric constant barium titanate ceramics subsequently.
In such scheme, described step 2) in, the particle diameter of barium titanate powder is 2 microns, and purity is 99.7%.
In such scheme, in described step 1), the concrete steps of ball milling are: the roller tank of load weighted chromium sesquioxide powder, aluminium powder, carbon dust, aluminum oxide powder and aluminum oxide abrading-ball being put into horizontal drum ball mill, ratio of grinding media to material is 2:1, and cylinder 24h obtains composite granule.
In such scheme, in described step 1), drying step is specially: composite granule is placed in to the vacuum drying oven inner drying 24h of 60 ℃.
In such scheme, described step 2) concrete steps that in, barium titanate powder are pressed into disk are: barium titanate powder is pressed into diameter 1.5cm under the pressure of 200MPa, the disk of height 0.8cm.
In such scheme, described step 2) in, be pressed into barium titanate just the concrete steps of base be: under the pressure of 8MPa, be pressed into diameter 2cm, the barium titanate of height 1.0cm is base just.
In such scheme, the height of the column in described step 3) is 5cm, and diameter is 7cm.
Principle of the present invention is: the present invention adopts self propagating high temperature Quick-pressing sintering technology, will work as self-propagating reaction just to complete, and built-in barium titanate just base still when red soft state, apply fast a large pressure, once complete the densification process of barium titanate ceramics.From spreading system, be here aluminothermy system, because aluminium powder has compared with strong reducing property, this system can produce reducing atmosphere after igniting, under high temperature reduction atmosphere, the inside crystal grain of barium titanate ceramics material becomes semi-conductivity because of a small amount of Sauerstoffatom loss, and crystal boundary is because reoxidizing in temperature-fall period becomes insulation layer.When crystal grain has semi-conductivity, when crystal boundary has insulativity, under DC Electric Field, electronics in crystal grain will jump near crystal boundary, and accumulate near crystal boundary, form numerous little electric capacity, thereby can form crystal boundary barrier-layer effect, and cause barium titanate ceramics to present very high specific inductivity on apparent.
Compared with prior art, beneficial effect of the present invention is as follows:
The first, without barium carbonate powder being carried out to any processing, just can prepare that to have specific inductivity high, dielectric loss is low, and degree of compactness is high, the barium titanate ceramics that thermostability is high.
The second, adopt self propagating high temperature Quick-pressing sintering technology, compare with conventional sintering means, have heat-up rate fast, sintering time is short, and low advantage consumes energy.
The 3rd, for the powder certainly spreading, be industrial rank, for purity and particle diameter, have no special requirements, therefore can reduce production costs.
The 4th, the method technique is simple, and preparation cycle is short, is conducive to realize industrialized mass.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the embodiment of the present invention 1 gained huge dielectric constant barium titanate ceramics.
Fig. 2 is the SEM figure of the embodiment of the present invention 1 gained huge dielectric constant barium titanate ceramics.
Fig. 3 is the dielectric thermogram of the embodiment of the present invention 1 gained huge dielectric constant barium titanate ceramics.
Embodiment
In order to understand better the present invention, below in conjunction with embodiment and accompanying drawing, further illustrate content of the present invention, but content of the present invention is not only confined to the following examples.
embodiment 1:
The present embodiment provides a kind of preparation method of huge dielectric constant barium titanate ceramics, and it comprises the following steps:
1) preparation is from spreading system powder
1. by weight percentage, take this system and need chromium sesquioxide powder 109.55g, aluminium powder 38.92g, carbon dust 11.53g, aluminum oxide powder 40.00g, load weighted chromium sesquioxide powder, aluminium powder, carbon dust, aluminum oxide powder and aluminum oxide abrading-ball are put into the roller tank of horizontal drum ball mill, ratio of grinding media to material is 2:1, and cylinder 24h obtains composite granule.
2. composite granule is placed in to 24h in 60 ℃ of vacuum drying ovens, crosses 50 mesh sieve granulations, obtain granular composite granule.
2) prepare just base of barium titanate
1. under the pressure of 200MPa, barium titanate powder (particle diameter is 2 microns, and purity is 99.7%) is pressed into diameter 1.5cm, the disk of height 0.8cm.
2. barium titanate disk is wrapped up to one deck graphite paper, then wrap up the boron nitride powder of 1g, be pressed into diameter 2cm under the pressure of 8MPa, the barium titanate of height 1.0cm is base just.
3) self propagating high temperature Quick-pressing sintering: the first base of barium titanate is positioned in the composite granule making through step 1), is pressed into column (height 5cm, diameter 7cm) under 8MPa pressure.Column is positioned in self propagating high temperature Quick-pressing equipment, with the tungsten filament self-propagating reaction that ignites, and in the time of 70 seconds, applies the axle pressure of 200MPa, pressurize 60 seconds, naturally cooling, obtains huge dielectric barium titanate pottery subsequently.
The performance of gained barium titanate ceramics sample is as follows: relative density 99.7%, and under room temperature 1KHz, relative permittivity is 75000, dielectric loss is 5%, between 50 ℃～250 ℃, the velocity of variation (ε of dielectric constant with temperature
max-ε
min)/ε
maxbe 14%.
Wherein, the measuring method of above-mentioned relative density is as follows: general ventilate and the inner hole of holding one's breath being communicated with that exist in ceramic sample, the apparent density of measure sample used, apparent density=sample mass/(actual volume+ventilate volume+pore volume of holding one's breath of sample), can all include nearly all pore in sample.Adopt apparent density to calculate relative density and can calculate density comparatively accurately.Apparent density and relative density are calculated formula:
Wherein, ρ-apparent density; ρ
waterthe density of-water, W
1the aerial quality of-sample; W
2-sample is immersed in the quality in water; W
3the aerial quality of sample after-immersion; ρ
verythe true density of-barium titanate.
As seen from Figure 1, prepared barium titanate ceramics are pure phase, not containing any impurity.75 ° of left and right, there is bimodal distribution corresponding (103), (301) crystal face in diffraction peak; 79 ° of left and right, also occur bimodal distribution, corresponding (113), (311) crystal face, proved in barium titanate ceramics and obviously had Tetragonal to exist.
As seen from Figure 2, gained barium titanate ceramics are completely fine and close, and sample relative density is higher.Crystal grain median size is 20 m left and right, and pore-free exists.
As seen from Figure 3, the specific inductivity of gained barium titanate ceramics is along with temperature raises and raises.And, even if the specific inductivity of gained barium titanate ceramics keeps higher numerical value at the frequent energy of height.
embodiment 2
The present embodiment provides a kind of preparation method of huge dielectric constant barium titanate ceramics, and it comprises the following steps:
1) preparation is from spreading system powder
1. by weight percentage, take this system and need chromium sesquioxide powder 110.35g, aluminium powder 40.15g, carbon dust 12.50g, aluminum oxide powder 37.00g, load weighted chromium sesquioxide powder, aluminium powder, carbon dust, aluminum oxide powder and aluminum oxide abrading-ball are put into the roller tank of horizontal drum ball mill, ratio of grinding media to material is 2:1, and cylinder 24h obtains composite granule.
2. composite granule is placed in to 24h in 60 ℃ of vacuum drying ovens, crosses 50 mesh sieve granulations, obtain granular composite granule.
2) prepare just base of barium titanate
1. under the pressure of 200MPa, barium titanate powder (particle diameter is 2 microns, and purity is 99.7%) is pressed into diameter 1.5cm, the disk of height 0.8cm.
2. barium titanate disk is wrapped up to one deck graphite paper, then wrap up the boron nitride powder of 1g, be pressed into diameter 2cm under the pressure of 8MPa, the barium titanate of height 1.0cm is base just.
3) self propagating high temperature Quick-pressing sintering: the first base of barium titanate is positioned in the composite granule making through step 1), is pressed into column (height 5cm, diameter 7cm) under 8MPa pressure.Column is positioned in self propagating high temperature Quick-pressing equipment, with the tungsten filament self-propagating reaction that ignites, and in the time of 40 seconds, applies the axle pressure of 200MPa, pressurize 60 seconds, naturally cooling, obtains huge dielectric barium titanate pottery subsequently.
The performance of gained barium titanate ceramics sample is as follows: relative density 96.3%, and under room temperature 1KHz, relative permittivity is 58000, dielectric loss is 3.5%, between 50 ℃～250 ℃, the velocity of variation (ε of dielectric constant with temperature
max-ε
min)/ε
maxbe 20%.
embodiment 3
The present embodiment provides a kind of preparation method of huge dielectric constant barium titanate ceramics, and it comprises the following steps:
1) preparation is from spreading system powder
1. by weight percentage, take this system and need chromium sesquioxide powder 123.24g, aluminium powder 43.78g, carbon dust 12.94g, aluminum oxide powder 20.00g, load weighted chromium sesquioxide powder, aluminium powder, carbon dust, aluminum oxide powder and aluminum oxide abrading-ball are put into the roller tank of horizontal drum ball mill, ratio of grinding media to material is 2:1, and cylinder 24h obtains composite granule.
2. composite granule is placed in to 24h in 60 ℃ of vacuum drying ovens, crosses 50 mesh sieve granulations, obtain granular composite granule.
2) prepare just base of barium titanate
1. under the pressure of 200MPa, barium titanate powder (particle diameter is 2 microns, and purity is 99.7%) is pressed into diameter 1.5cm, the disk of height 0.8cm.
2. barium titanate disk is wrapped up to one deck graphite paper, then wrap up the boron nitride powder of 1g, be pressed into diameter 2cm under the pressure of 8MPa, the barium titanate of height 1.0cm is base just.
3) self propagating high temperature Quick-pressing sintering: the first base of barium titanate is positioned in the composite granule making through step 1), is pressed into column (height 5cm, diameter 7cm) under 8MPa pressure.Column is positioned in self propagating high temperature Quick-pressing equipment, with the tungsten filament self-propagating reaction that ignites, and in the time of 50 seconds, applies the axle pressure of 100MPa, pressurize 60 seconds, naturally cooling, obtains huge dielectric barium titanate pottery subsequently.
The performance of gained barium titanate ceramics sample is as follows: relative density 98.6%, and under room temperature 1KHz, relative permittivity is 67000, dielectric loss is 4.2%, between 50 ℃～250 ℃, the velocity of variation (ε of dielectric constant with temperature
max-ε
min)/ε
maxbe 16%.
Relative density, relative permittivity, the dielectric loss of the huge dielectric barium titanate pottery that embodiment of the present invention 1-3 is prepared are as shown in table 1:
Table 1
| Embodiment | Alumina content | Clamping time | Relative density | Relative permittivity | Dielectric loss | Temperature coefficient of capacitance |
| Embodiment 1 | 20% | 70s | 99.7% | 75000 | 5% | 14% |
| Embodiment 2 | 18.5% | 40s | 96.3% | 58000 | 3.5% | 20% |
| Embodiment 3 | 10% | 50s | 98.6% | 67000 | 4.2% | 16% |
As can be seen from Table 1, the barium titanate ceramics that a process for preparing have highly dense solidity (>96%), high relative permittivity (>58000), low dielectric loss (<5%), low temperature coefficient of capacitance (<20%), illustrates that adopted self propagating high temperature quick pressure prepares huge dielectric barium titanate pottery and have larger advantage; In addition, can find out, along with the postponement of clamping time, the relative density of pottery improves, and relative permittivity also increases; Moreover the change of alumina content also has impact to ceramic performance, this is because aluminum oxide is a kind of thinner in certainly spreading system, can control the temperature of self-propagating reaction, thereby controls ceramic degree of compactness.
The first base of barium titanate can be avoided and the pollution of aluminothermy system bonding with the isolation of graphite paper parcel, and while graphite has good thermal conductivity.Use boron nitride wrap up to be for barium titanate after guaranteeing to pressurize can be not cracked and block can be not cracked when taking-up barium titanate ceramics.
Each cited raw material of the present invention can be realized the present invention, the bound value of each raw material with and interval value can realize the present invention, the bound value of processing parameter of the present invention (as proportioning, temperature, time etc.) with and interval value can realize the present invention, at this, do not enumerate embodiment.
Claims (7)
1. a preparation method for huge dielectric constant barium titanate ceramics, is characterized in that, it comprises the following steps:
1) preparation is from spreading system powder
By weight percentage, take chromium sesquioxide powder 54%-62%, aluminium powder 19%-22%, carbon dust 5%-7%, aluminum oxide powder 10%-20%, carries out ball milling by load weighted chromium sesquioxide powder, aluminium powder, carbon dust, aluminum oxide powder after mixing, and obtains composite granule;
Composite granule is dried, and granulation, obtains granular composite granule;
2) prepare just base of barium titanate
Barium titanate powder is pressed into disk, then barium titanate disk is superscribed to graphite paper and boron nitride powder successively, be then pressed into just base of barium titanate, the particle diameter of described barium titanate powder is 2 microns;
3) self propagating high temperature Quick-pressing sintering:
The first base of barium titanate is positioned in the granular composite granule making through step 1), be pressed into column, described column is positioned in self propagating high temperature Quick-pressing equipment, self-propagating reaction ignites, and in the time of 40 seconds-70 seconds, apply the axle pressure of 100MPa-200MPa, pressurize 60 seconds, naturally cooling, obtains huge dielectric constant barium titanate ceramics subsequently.
2. preparation method as claimed in claim 1, is characterized in that, described step 2) in the purity of barium titanate powder be 99.7%.
3. preparation method as claimed in claim 1, it is characterized in that, in described step 1), the concrete steps of ball milling are: the roller tank of load weighted chromium sesquioxide powder, aluminium powder, carbon dust, aluminum oxide powder and aluminum oxide abrading-ball being put into horizontal drum ball mill, ratio of grinding media to material is 2:1, and cylinder 24h obtains composite granule.
4. preparation method as claimed in claim 1, is characterized in that, in described step 1), drying step is specially: composite granule is placed in to the vacuum drying oven inner drying 24h of 60 ℃.
5. preparation method as claimed in claim 1, is characterized in that, described step 2) in barium titanate powder is pressed into disk concrete steps be: barium titanate powder is pressed into diameter 1.5cm under the pressure of 200MPa, the disk of height 0.8cm.
6. preparation method as claimed in claim 1, is characterized in that, described step 2) in be pressed into barium titanate just the concrete steps of base be: under the pressure of 8MPa, be pressed into diameter 2cm, the barium titanate of height 1.0cm is base just.
7. preparation method as claimed in claim 1, is characterized in that, the height of the column in described step 3) is 5cm, and diameter is 7cm.
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| CN115073165B (en) * | 2022-06-17 | 2023-08-04 | 桂林电子科技大学 | Giant dielectric constant BaTiO 3 Ceramic and preparation method thereof |
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| CN101343179A (en) * | 2008-08-15 | 2009-01-14 | 天津大学 | Low-loss high-frequency medium ceramic and preparation thereof |
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Non-Patent Citations (4)
| Title |
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| Fabrication of ultrafine-grained alumina ceramics by two different fast sintering methods;Fancheng Meng等;《Ceramics International》;20110329;第37卷;1973－1977 * |
| Fan Zhang等.Ultra-fast densification of boron carbide ceramics under high heating rate and high pressure.《Ceramics International》.2010,第36卷1491－1494. |
| Fancheng Meng等.Fabrication of ultrafine-grained alumina ceramics by two different fast sintering methods.《Ceramics International》.2011,第37卷1973－1977. |
| Ultra-fast densification of boron carbide ceramics under high heating rate and high pressure;Fan Zhang等;《Ceramics International》;20100301;第36卷;1491－1494 * |
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